Mediated electroreduction of Au(I) using C70 fullerene, methano[60]fullerene and [60]fulleropyrrolidine as a mediator at the potentials of mediator reduction to the radical anion was used to obtain nanocomposites of gold nanoparticles (AuNP) with mediator in toluene-DMF (2:1, by volume)/0.1 M Bu4NCl medium. The nanocomposite consists of AuNP bound by fullerene to aggregates that are dispersed in a fullerene matrix. The aggregates have the form of a “flower”. Size of aggregates (from 55 ± 17 to 95 ± 22 nm), AuNP (from 10 ± 1 to 19 ± 5 nm), metal crystallites (from 6 to 16 nm) depends on the nature of a mediator, and this dependence for aggregates and AuNP is antibate. The electrolysis occurs efficiently in all cases, and Au(I) is mediately quantitatively reduced to Au(0) with the formation of nanoparticles, and ultimately their aggregates, upon consumption of the theoretical amount of electricity. Metal and nanocomposite are not deposited in appreciable quantities on the electrode and are almost completely stabilized in the solution bulk. All the particles were characterized by electron microscopy methods (SEM, HR TEM) and X-ray powder diffraction (XRPD).